Kinetic and Magic Angle Spinning-Nuclear Magnetic Resonance Studies of Dry Oxidation of Beta-Sialon Powders

Hajime Kiyono, Shiro Shimada

Research output: Contribution to journalArticle

5 Citations (Scopus)

Abstract

The oxidation of α-Si3N4 and β-sialon (Si6-z AlzOzN8-z) powders with the different z values (z = 1, 2, 3) in a dry atmosphere of Ar/O2 (80/20 kPa) at 1000-1300°C was studied by X-ray diffraction, 29Si and 27Al magic-angle spinning-nuclear magnetic resonance (MAS-NMR), transmission electron microscopy (TEM), and thermogravimetric analysis. The oxidation products of the β-sialons consisted of amorphous SiO2 and aluminosilicate, the latter crystallizing to mullite at T ≥ 1200°C. Very fine acicular mullite grains were formed in the oxidized particles as confirmed by TEM. The initial oxidation kinetics can be described by a two-stage linear law for a degree of reaction less than 10%, followed by parabolic oxidation at 10-60% reaction. In both the linear and parabolic kinetic regions, the oxidation rate constants were very similar for the three sialons but were smaller for α-Si3N4. The activation energies for the linear kinetic regions were 260, 260, 300, and 270 kJ mol 1 for α-Si3N4 and the β-sialons with z = 1, 2, and 3, respectively, whereas the corresponding values for the diffusion process were 410, 430, 410, and 380 kJ mol 1. The oxidation mechanism is discussed on the basis of the X-ray diffraction, 29Si and 27Al MAS-NMR, and kinetic results.

Original languageEnglish
JournalJournal of the Electrochemical Society
Volume148
Issue number2
DOIs
Publication statusPublished - 2001
Externally publishedYes

Fingerprint

sialon
Magic angle spinning
Powders
metal spinning
Nuclear magnetic resonance
Oxidation
nuclear magnetic resonance
oxidation
Kinetics
kinetics
Mullite
Transmission electron microscopy
X ray diffraction
transmission electron microscopy
Aluminosilicates
diffraction
Thermogravimetric analysis
Rate constants
x rays
Activation energy

ASJC Scopus subject areas

  • Electrochemistry
  • Surfaces, Coatings and Films
  • Surfaces and Interfaces

Cite this

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title = "Kinetic and Magic Angle Spinning-Nuclear Magnetic Resonance Studies of Dry Oxidation of Beta-Sialon Powders",
abstract = "The oxidation of α-Si3N4 and β-sialon (Si6-z AlzOzN8-z) powders with the different z values (z = 1, 2, 3) in a dry atmosphere of Ar/O2 (80/20 kPa) at 1000-1300°C was studied by X-ray diffraction, 29Si and 27Al magic-angle spinning-nuclear magnetic resonance (MAS-NMR), transmission electron microscopy (TEM), and thermogravimetric analysis. The oxidation products of the β-sialons consisted of amorphous SiO2 and aluminosilicate, the latter crystallizing to mullite at T ≥ 1200°C. Very fine acicular mullite grains were formed in the oxidized particles as confirmed by TEM. The initial oxidation kinetics can be described by a two-stage linear law for a degree of reaction less than 10{\%}, followed by parabolic oxidation at 10-60{\%} reaction. In both the linear and parabolic kinetic regions, the oxidation rate constants were very similar for the three sialons but were smaller for α-Si3N4. The activation energies for the linear kinetic regions were 260, 260, 300, and 270 kJ mol 1 for α-Si3N4 and the β-sialons with z = 1, 2, and 3, respectively, whereas the corresponding values for the diffusion process were 410, 430, 410, and 380 kJ mol 1. The oxidation mechanism is discussed on the basis of the X-ray diffraction, 29Si and 27Al MAS-NMR, and kinetic results.",
author = "Hajime Kiyono and Shiro Shimada",
year = "2001",
doi = "10.1149/1.1339865",
language = "English",
volume = "148",
journal = "Journal of the Electrochemical Society",
issn = "0013-4651",
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T1 - Kinetic and Magic Angle Spinning-Nuclear Magnetic Resonance Studies of Dry Oxidation of Beta-Sialon Powders

AU - Kiyono, Hajime

AU - Shimada, Shiro

PY - 2001

Y1 - 2001

N2 - The oxidation of α-Si3N4 and β-sialon (Si6-z AlzOzN8-z) powders with the different z values (z = 1, 2, 3) in a dry atmosphere of Ar/O2 (80/20 kPa) at 1000-1300°C was studied by X-ray diffraction, 29Si and 27Al magic-angle spinning-nuclear magnetic resonance (MAS-NMR), transmission electron microscopy (TEM), and thermogravimetric analysis. The oxidation products of the β-sialons consisted of amorphous SiO2 and aluminosilicate, the latter crystallizing to mullite at T ≥ 1200°C. Very fine acicular mullite grains were formed in the oxidized particles as confirmed by TEM. The initial oxidation kinetics can be described by a two-stage linear law for a degree of reaction less than 10%, followed by parabolic oxidation at 10-60% reaction. In both the linear and parabolic kinetic regions, the oxidation rate constants were very similar for the three sialons but were smaller for α-Si3N4. The activation energies for the linear kinetic regions were 260, 260, 300, and 270 kJ mol 1 for α-Si3N4 and the β-sialons with z = 1, 2, and 3, respectively, whereas the corresponding values for the diffusion process were 410, 430, 410, and 380 kJ mol 1. The oxidation mechanism is discussed on the basis of the X-ray diffraction, 29Si and 27Al MAS-NMR, and kinetic results.

AB - The oxidation of α-Si3N4 and β-sialon (Si6-z AlzOzN8-z) powders with the different z values (z = 1, 2, 3) in a dry atmosphere of Ar/O2 (80/20 kPa) at 1000-1300°C was studied by X-ray diffraction, 29Si and 27Al magic-angle spinning-nuclear magnetic resonance (MAS-NMR), transmission electron microscopy (TEM), and thermogravimetric analysis. The oxidation products of the β-sialons consisted of amorphous SiO2 and aluminosilicate, the latter crystallizing to mullite at T ≥ 1200°C. Very fine acicular mullite grains were formed in the oxidized particles as confirmed by TEM. The initial oxidation kinetics can be described by a two-stage linear law for a degree of reaction less than 10%, followed by parabolic oxidation at 10-60% reaction. In both the linear and parabolic kinetic regions, the oxidation rate constants were very similar for the three sialons but were smaller for α-Si3N4. The activation energies for the linear kinetic regions were 260, 260, 300, and 270 kJ mol 1 for α-Si3N4 and the β-sialons with z = 1, 2, and 3, respectively, whereas the corresponding values for the diffusion process were 410, 430, 410, and 380 kJ mol 1. The oxidation mechanism is discussed on the basis of the X-ray diffraction, 29Si and 27Al MAS-NMR, and kinetic results.

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